Triethylamine → HCID 54040071、化合物

HRID 233742

反応式

HRID 233742 の反応式
CC([O-])(C)C.[K+].Cl.[NH2:8][C@@H:9]([CH2:14][CH2:15][CH2:16]C)[C:10]([O:12][CH3:13])=[O:11].C(N(CC)CC)C.[Br:25][C:26]1[CH:31]=[CH:30][C:29]([CH2:32]Br)=[CH:28][N:27]=1>COCCOC.CN(C=O)C>[Br:25][C:26]1[N:27]=[CH:28][C:29]([CH2:32][NH:8][C@H:9]([C:10]([O:12][CH3:13])=[O:11])[CH2:14][CH2:15][CH3:16])=[CH:30][CH:31]=1

参加物

7

反応物 4

HCID 8471TriethylamineHCID 64246602-Bromo-5-bromomethylpyridineHCID 14039065methyl (2S)-2-aminohexanoate hydrochlorideHCID 23665647Potassium tert-butoxide

生成物 1

HCID 54040071HCID 54040071、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒2 回HCID 80711,2-Dimethoxyethane溶媒

反応条件

温度
20 °C

実験手順

1.48 g (13.2 mmol) of potassium tert-butylate are added to a solution of 2.18 g (12 mmol) of methyl (S)-2-aminohexanoate hydrochloride and 1.66 ml of triethylamine in 20 ml of DME and 15 ml of DMF under argon. After stirring at 20° C. for 1 h, a solution of 3.01 g (12 mmol) of 2-bromo-5-bromomethylpyridine in 15 ml of DMF is injected and the mixture is stirred for 16 h. Subsequently, the solvent is distilled off in vacuo and the residue is taken up in dichloromethane/water; the organic phase is then dried over sodium sulphate and, after concentrating, purified on silica gel using petroleum ether/ethyl acetate (4:1).

後処理

  1. stirringthe mixture is stirred for 16 h
  2. distillationSubsequently, the solvent is distilled off in vacuo
  3. dry with materialthe organic phase is then dried over sodium sulphate
  4. concentrationafter concentrating
  5. custompurified on silica gel

出典と根拠

ORDレコード
ord-e392811c6725432ca09c3d03f743034d
出典データセット
uspto-grants-1997_01
特許番号
US05594010

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